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A kind of cage type polysilsesquioxane containing phenylethynyl group and its synthesis method and application

A technology based on polysilsesquioxane and phenylethynyl, which is applied in the field of polysilsesquioxane synthesis, can solve the problems of high-molecular material performance impact, material performance degradation, and poor miscibility, etc., and achieve excellent antigenicity Effects of oxygen characteristics, low melting temperature, and low dielectric characteristics

Active Publication Date: 2022-08-02
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, when POSS is used to improve the performance of other polymer materials by blending in the prior art, there is a phase separation phenomenon caused by poor miscibility, which will lead to a decrease in material performance; and when POSS is introduced through copolymerization to improve the performance of polymer materials, The performance of polymer materials will also be affected by the content of POSS introduced

Method used

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  • A kind of cage type polysilsesquioxane containing phenylethynyl group and its synthesis method and application
  • A kind of cage type polysilsesquioxane containing phenylethynyl group and its synthesis method and application
  • A kind of cage type polysilsesquioxane containing phenylethynyl group and its synthesis method and application

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[0046] The invention provides a method for synthesizing phenylethynyl-containing cage-type polysilsesquioxane, which comprises the following steps:

[0047] (1) 4-phenylethynyl phthalic anhydride with the A group, N-[(heptaisobutyl POSS) propyl]-3,5-diaminobenzamide and an organic solvent are added to the reactor to carry out react to obtain a mixed solution comprising the phenylethynyl-containing cage polysilsesquioxane;

[0048] (2) post-processing the mixed solution obtained in step (1) to obtain the cage-type polysilsesquioxane containing phenylethynyl groups;

[0049] Wherein, the structural formula of described N-[(heptaisobutyl POSS) propyl]-3,5-diaminobenzamide is shown in (II):

[0050]

[0051] In the present invention, the use of amino-containing cage polysilsesquioxane (ie N-[(heptaisobutyl POSS) propyl]-3,5-diaminobenzamide) and phenylethynyl phthalic anhydride using high temperature One-step imidization method, that is, through condensation polymerization of...

Embodiment 1

[0078] Example 1: Synthesis of phenylethynyl-containing cage polysilsesquioxane

[0079] (1) Add 24.842g (0.1mol) 4-phenylethynyl phthalic anhydride, 25.218g (0.025mol) N-[(heptaisobutyl POSS)propyl]-3,5-diaminobenzene into a three-necked round-bottomed flask Formamide and 300.36g nitrogen nitrogen dimethylformamide (DMF), connect the three-necked flask to a nitrogen protection device and a reflux condensing device, then add it to an oil bath at 160 ° C, and heat under reflux for 8 hours to obtain the target compound (that is, Mixed solution of cage-type polysilsesquioxane containing phenylethynyl group);

[0080] (2) utilize underpressure distillation apparatus to carry out underpressure distillation to the mixed solution that step (1) obtains, stop underpressure distillation when remaining concentrated solution quality is 87g, obtain concentrated solution;

[0081] The concentrated solution was added to a single-neck flask containing 350 g of absolute ethanol, and the react...

Embodiment 2

[0083] Example 2: Synthesis of phenylethynyl-containing cage polysilsesquioxane

[0084] (1) Add 13.663g (0.055mol) 4-phenylethynyl phthalic anhydride, 25.218g (0.025mol) N-[(heptaisobutyl POSS)propyl]-3,5-diaminobenzene into a three-necked round-bottomed flask Formamide and 155.53 g of nitrogen nitrogen dimethylformamide (DMF), connect the three-necked flask to a nitrogen protection device and a reflux condenser, then add it to an oil bath at 160 ° C, and heat under reflux for 6 h to obtain the target compound (that is, Mixed solution of cage-type polysilsesquioxane containing phenylethynyl group);

[0085] (2) utilize underpressure distillation apparatus to carry out underpressure distillation to the mixed solution that step (1) obtains, stop underpressure distillation when remaining concentrated solution quality is 64.4g, obtain concentrated solution;

[0086] The concentrated solution was added to a single-necked flask containing 128.8 g of absolute ethanol, and the react...

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Abstract

The invention provides a cage-type polysilsesquioxane containing a phenylethynyl group and a synthesis method and application thereof. The cage-type polysilsesquioxane has the structure shown in (I): wherein the R group is an A group, and the method comprises: combining 4-phenylethynyl phthalic anhydride, N-[(heptaisobutyl POSS) propyl group]-3,5-diaminobenzamide joins in organic solvent and reacts, then underpressure distillation, then in alcoholic solvent, heating and refluxing removes unreacted 4-phenylethynyl phthalic anhydride to obtain the described Cage polysilsesquioxane containing phenylethynyl groups. The invention also provides the application of the phenylethynyl group-containing cage polysilsesquioxane in the preparation of thermosetting macromolecular polymers. The phenylacetylene group-containing cage polysilsesquioxane of the present invention can be directly crosslinked by heating to form a thermosetting polymer with high temperature resistance, atomic oxygen resistance and low dielectric properties.

Description

technical field [0001] The invention relates to the technical field of polysilsesquioxane synthesis, in particular to a cage-type polysilsesquioxane containing a phenylethynyl group and a synthesis method and application thereof. Background technique [0002] Cage polysilsesquioxane (POSS) is a kind of cage-like compound connected by silicon-oxygen bonds. The rich silicon-oxygen content endows it with excellent atomic oxygen resistance and high temperature resistance. The structure makes it bulky and low-dielectric. The organic groups attached to the surface of the POSS silica cage endow its properties and structure with tunability to improve its compatibility with the organic polymer resin matrix. In the prior art, POSS is introduced into other high-molecular polymers as a polymerized monomer or an additive by means of copolymerization / blending, which can improve the performance of the high-molecular material. [0003] At present, when POSS is blended to improve the prope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/388C08L83/08
CPCC08G77/045C08L83/08
Inventor 王振合张春波袁航谢非张昊
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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